CN112272602A - Process for preparing coloured polymer compositions - Google Patents

Process for preparing coloured polymer compositions Download PDF

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Publication number
CN112272602A
CN112272602A CN201980037991.1A CN201980037991A CN112272602A CN 112272602 A CN112272602 A CN 112272602A CN 201980037991 A CN201980037991 A CN 201980037991A CN 112272602 A CN112272602 A CN 112272602A
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Prior art keywords
solvent
mold release
polymer
release agent
pigment
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CN201980037991.1A
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CN112272602B (en
Inventor
J·彼得简安东尼
T·M·艾根汇森
B·维恩范
J·A·范登伯格
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SABIC Global Technologies BV
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SABIC Global Technologies BV
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22—Component parts, details or accessories; Auxiliary operations
    • B29B7/24—Component parts, details or accessories; Auxiliary operations for feeding
    • B29B7/242—Component parts, details or accessories; Auxiliary operations for feeding in measured doses
    • B29B7/244—Component parts, details or accessories; Auxiliary operations for feeding in measured doses of several materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/17—Articles comprising two or more components, e.g. co-extruded layers the components having different colours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/285—Feeding the extrusion material to the extruder
    • B29C48/288—Feeding the extrusion material to the extruder in solid form, e.g. powder or granules
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/94—Lubricating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/005—Processes for mixing polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/203—Solid polymers with solid and/or liquid additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3472—Five-membered rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B29B7/005—Methods for mixing in batches
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B29B7/007—Methods for continuous mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58—Component parts, details or accessories; Auxiliary operations
    • B29B7/60—Component parts, details or accessories; Auxiliary operations for feeding, e.g. end guides for the incoming material
    • B29B7/603—Component parts, details or accessories; Auxiliary operations for feeding, e.g. end guides for the incoming material in measured doses, e.g. proportioning of several materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2069/00—Use of PC, i.e. polycarbonates or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0005—Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
    • B29K2105/0032—Pigments, colouring agents or opacifiyng agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0018—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular optical properties, e.g. fluorescent or phosphorescent
    • B29K2995/002—Coloured
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/223—Packed additives

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The present invention relates to a process for preparing a coloured polymer composition comprising a polymer, a mould release agent and a colourant, the process comprising the steps of: feeding a mold release composition comprising the mold release agent and the colorant in solid form to a feed section of a melt mixing device; feeding the polymer to the melt mixing device; and mixing the mold release composition and the polymer in the melt mixing device at a temperature above the melting temperature of the polymer, wherein: -the colorant is a pigment or dye soluble in the release agent, -the polymer comprises or consists of polycarbonate, -the release agent is selected from the group consisting of pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate and mixtures thereof.

Description

Process for preparing coloured polymer compositions
The present invention relates to a process for preparing a coloured polymer composition comprising a polymer, a mould release agent and a colourant. The invention further relates to a method for producing semi-finished articles or batches of finished articles, to the use of a mold release composition in granular form and to a mold release composition.
Articles comprising or consisting of the colored polymeric compositions are generally prepared using a variety of techniques including sheet extrusion, profile extrusion, injection molding, blow molding, rotational molding, and compression molding. Generally these techniques involve the use of pre-formed colored polymer compositions containing polymers, colorants, mold release agents, and any other additives required for the intended application. Thus, in general, these techniques are primarily directed to the formation of pigmented polymer compositions rather than to the preparation of the compositions themselves. It is common in the polymer industry to make pigmented polymer compositions that can be used directly (i.e. without any additional modification) to form articles.
Another way of preparing a colored article of a colored polymer composition is to prepare a color concentrate or masterbatch and combine the base polymer composition with such color concentrate in situ (i.e., during the manufacture of the article). This generally allows more flexibility in changing the color of the article, but has the disadvantage of requiring multiple components to be used at the location of article manufacture, thereby making article manufacture more logistically complex and requiring article manufacturing equipment to allow more than one component to be handled.
In spite of the foregoing, an important aspect of colored articles is that these articles have some color consistency. Thus, it is desirable to minimize color variation between articles and within each individual article.
The colored polymer composition includes one or more colorants such as dyes and/or pigments. In view of the above color consistency, it is important that the pigment or dye is uniformly dispersed or dissolved within the polymer composition. In other words, color consistency requirements for the article can be translated into dispersing or dissolving pigments and/or dyes in the polymer composition.
US 5,116,547 discloses a method of coloring a polycarbonate extruded or molded product for an optical member by a liquid coloring method to obtain a colored polycarbonate extruded or molded product for an optical member by extrusion or injection molding. The method involves mixing a polycarbonate resin for an optical member and a liquid colorant dispersion obtained by dispersing a colorant in a dispersant. The dispersant includes a specific saturated fatty acid ester or silicone oil. After mixing the polycarbonate resin and the liquid colorant dispersion, the resulting mixture is melted and later extruded or molded to form a product for an optical member. Exemplary dispersants include butyl stearate, linseed oil, dimethyl polysiloxane, methyl phenyl polysiloxane, PE wax, paraffin wax and esters of alkylene oxides. The inventors have found that the liquid colouring process of US 5,116,547 is relatively complex and requires specific liquid feeding equipment to the extruder. Without wishing to be limited, the inventors further believe that feeding the liquid dispersion to the feed section of the extruder may cause instability in the formation of a stable melt within the extruder, which is defined by the inventors as "surging". In addition to this, the liquid feeding technique disclosed in US 5,116,547 may require precise pressure control within the feeding device.
US 2002/0013397 discloses a colored resin composition comprising a dispersant, a pigment and a thermoplastic resin; wherein the dispersant is represented by the formula CH2n+1(OCH2CH2)mOH and the thermoplastic resin is a metallocene polyolefin, wherein n is an integer of 1 to 100 and m is an integer of 1 to 100.
US 4,444,714 discloses a stable liquid gel useful for incorporating colorants in thermoplastic and thermosetting resins. The liquid gel comprises a liquid vehicle that is a plasticizer for the resin and is gelled by organophilic expanded lattice clay ion-exchanged with an alkylammonium ion.
WO2016/142447 discloses a masterbatch for colouring a thermoplastic polymer composition, said masterbatch comprising a colorant in a total amount of 10-50% (w/w) relative to the total weight of the masterbatch, a dispersant in a total amount of 0.5-20% (w/w) relative to the total weight of the masterbatch, and a carrier resin in a total amount of 30-80% (w/w) relative to the total weight of the masterbatch, wherein the dispersant is a polyol poly (hydroxy fatty acid) ester (pphe dispersant).
US 2014/0295160 discloses a method of producing a multilayer object having a dark glossy appearance, the method comprising the steps of: preparing a carbon-containing black master batch with a release agent; preparing a compound comprising polycarbonate and a carbon black-containing masterbatch, wherein the amount of carbon black is 0.05 to 0.15 wt% and the concentration of release agent is 0.1 to 0.5 wt%; producing a molded part; the mouldings are coated with the scratch-resistant layer in a first-stage coating process. The masterbatch in the examples was a carbon black/pentaerythritol tetrastearate masterbatch containing 58% carbon black.
EP 0365400 discloses a process for producing a filler-containing colored thermoplastic resin composition excellent in pigment dispersibility and impact resistance, which comprises first melt-kneading at least a part of the components of a resin composed of a thermoplastic resin (A) and/or a thermoplastic resin composition (B) with a filler (C), adding the remaining part of the resin (if present) and a pigment (E), and then further carrying out continuous melt-kneading.
US 2015/0344669 discloses a method of injection moulding an article having a thickness of between 1 and 3mm and having a b value in the CIE colour series between-1 and +0.1 and a haze value of less than 2% as measured at a 2mm thickness, the method comprising the steps of: a) providing a composition comprising i) a polyester produced by copolymerizing at least three monomers selected from the group consisting of at least one alkylene glycol and at least one dicarboxylic acid component in the presence of an aluminum or germanium compound, ii)1 to 5ppm of at least one dye, and iii)0.1 to 0.5 m% of a fatty acid ester mold release agent, and b) injecting the composition into a mold at a temperature below 60 ℃ until the mold is filled, and c) ejecting the article. This reference further discloses a composition comprising a) a polyester produced by copolymerizing 1, 2-ethylene glycol and two dicarboxylic acid components in the presence of a germanium compound, the dicarboxylic acid components comprising a terephthalic acid component and 4-20 mol% of an isophthalic acid component, the mol% being relative to the total amount of dicarboxylic acid components, characterized in that the composition further comprises B)0.2 to 1.5ppm of at least one dye, C)0.1 to 0.5 m% of stearyl stearate or glyceryl tristearate, and an article having a wall thickness between 1 and 3mm comprising the composition.
EP 0370424 discloses a resin composition for a masterbatch comprising 5 to 90% by weight of a modified polyolefin resin and 5 to 70% by weight of a carbon black having an average particle size of 15 to 120 μm and an oil absorption value of more than 50ml/100g, wherein the volatile component is less than 3.5% by weight.
It is an object of the present invention to provide a process for preparing a coloured polymer composition which allows the manufacture of articles having improved colour consistency.
It is a further object of the present invention to provide a process for preparing a coloured polymer composition which is cost-effective and does not require major modifications to existing equipment, such as in particular extruders.
In particular, it is an object of the present invention to provide a cost-effective and robust method for preparing colored polycarbonate compositions, which method allows for the manufacture of polycarbonate articles with improved color consistency.
One or more of these objects are at least partially achieved according to the present invention, which relates to a process for preparing a coloured polymer composition comprising at least one polymer, a mould release agent and a colorant, the process comprising the steps of: feeding a mold release composition comprising the mold release agent and the colorant in solid form to a feed section of a melt mixing device; feeding the polymer to the melt mixing device; and mixing the mold release composition and the polymer in the melt mixing device at a temperature above the melting temperature of the polymer, wherein:
-the colorant is a pigment or dye soluble in the release agent,
-the polymer comprises or consists of polycarbonate,
-the mould release agent is selected from the group consisting of pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate and mixtures thereof.
The present inventors have surprisingly found that such a process will result in polymer compositions, particularly polycarbonate compositions, that exhibit improved color consistency.
The present invention relates to compositions based on polycarbonate. Thus, the polymer in the composition comprises or consists of polycarbonate. If the polymer comprises polycarbonate, the amount of polycarbonate is preferably at least 60 wt.%, preferably at least 80 wt.%, more preferably at least 90 wt.%, based on the weight of the polymer. That is, the polymer comprises a major portion of polycarbonate and a minor portion of other polymers (if present). For example, the polymer may be a mixture of polycarbonate and one or more of polyethylene terephthalate, polybutylene terephthalate, polymethyl methacrylate, polyester copolymers, acrylonitrile-butadiene-styrene copolymers, styrene acrylonitrile copolymers. For the avoidance of doubt, polycarbonate copolymers or polyester-co-carbonate polymers are considered polycarbonates.
In a preferred embodiment, the polymer comprises or consists of an aromatic polycarbonate or a mixture of at least two aromatic polycarbonates. Similarly, in the above blends, the polycarbonate is preferably an aromatic polycarbonate. Preferably, the aromatic polycarbonate is a bisphenol a derived polycarbonate. Bisphenol a-derived polycarbonates are well known to the skilled artisan and can be prepared by a melt transesterification process involving the transesterification of bisphenol a and diphenyl carbonate, or by an interfacial process involving the reaction of phosgene with bisphenol a. Such polycarbonates are generally referred to as polycarbonate homopolymers.
In one embodiment, the polycarbonate is a polycarbonate copolymer or a mixture of a polycarbonate copolymer and a polycarbonate homopolymer. Polycarbonate copolymers are known per se, and examples include polyorganosiloxanes, block copolymers such as polydimethylsiloxane and polycarbonate. If the polycarbonate is a mixture of a polycarbonate copolymer and a polycarbonate homopolymer, the amount of polycarbonate homopolymer may be at least 80 wt.%, preferably at least 90 wt.%, more preferably at least 95 wt.% of polycarbonate homopolymer based on the total weight of the polycarbonate polymer.
Despite the preferred polymers mentioned above, other polymers that can be applied in the present invention are polyethylene, polypropylene, ethylene propylene copolymers, propylene ethylene copolymers, ethylene (meth) acrylate copolymers, polyvinyl chloride, polyamides, polyetherimides, polyetheretherketones and polyvinylsulfones. Such polymers, if present, will by definition form a minor portion of the polymers in the composition.
The polymer composition comprises a polymer, a mold release agent, and a colorant. Preferably, the amount of mold release agent is from 0.01 to 1.0 wt% and the amount of colorant is from 0.1 to 1000ppm by weight, based on the weight of the sum of polymer, mold release agent, and colorant in the polymer composition.
Preferably, the amount of mold release agent is from 0.1 to 1.0 wt%, more preferably from 0.3 to 0.8 wt%, based on the weight of the sum of polymer, mold release agent and colorant in the polymer composition. If the amount of release agent is too high, it may result in undesirable deposition of the release agent on the die, chill roll, calender roll or extrusion die, requiring more frequent cleaning and thus reduced throughput. Other properties such as impact performance and flame retardancy may also be affected. If the amount of the release agent is too low, the release property of the polymer composition is insufficient.
The amount of colorant is generally selected to achieve the desired color intensity. The amount of colorant in the polymer composition may be from 0.1 to 1000ppm by weight.
The polymer composition may comprise further additives and/or fillers, such as inorganic fillers.
The colorant may be a pigment or dye suitable for providing the desired shade to the polymer. The skilled person knows how to select an appropriate colorant based on the type of polymer. In the context of the present invention, the colorant should be soluble in the mold release agent. The insoluble colorant may exude the mold release agent over time, causing undesirable problems in storage or transportation of the mold release composition, contaminating the feed section (or any other transportation section, such as a pipeline) of or near the melt mixing device, and/or making the color shade of articles produced based on the colored mold release composition inconsistent.
In other words, the colorant is a pigment or dye that is soluble in the applied release agent. It is preferred that the colorant is a dye that is soluble in the mold release agent, as this allows for the preparation of a stable mold release composition, i.e., a mold release composition in which the amount of colorant is stable over time.
Useful pigments may include, for example: inorganic pigments such as metal oxides and mixed metal oxides such as zinc oxide, titanium dioxide, iron oxides, or the like; sulfides such as zinc sulfide or the like; an aluminate salt; sodium sulfosilicate sulfate, chromate, or the like; zinc ferrite; ultramarine; organic pigments such as azo, diazo, quinacridone, perylene, naphthalene tetracarboxylic acid, xanthenone, isoindolinone, tetrachloroisoindolinone, anthraquinone, enthrones, dioxazine, phthalocyanine and azo lakes; pigment red 101, pigment red 122, pigment red 149, pigment red 177, pigment red 179, pigment red 202, pigment violet 29, pigment blue 15, pigment blue 60, pigment green 7, pigment yellow 119, pigment yellow 147, pigment yellow 150 and pigment brown 24; or combinations comprising at least one of the foregoing pigments. Preferably, organic pigments are used in preference to inorganic pigments, and preferably the colorant does not contain inorganic pigments.
More preferably, however, the colorant is a dye that is soluble in the mold release agent. The dyes can belong to methane type, anthraquinone type, perylene type, thioindigo type, phthalocyanine type, coumarin type, dibenzoxazolyl phthalate type or oxazolstilbene type. Examples of organic dyes which can be used are triphenylmethane, oxazine, thiazine, nitromethine, azo dyes and anthraquinone dyes. Mention may be made, among azo dyes, for example, of diazo dyes and in particular monoazo dyes, such as, for example, dyes of the phenylazobenzene, phenylazopyrazolinone, phenylazoacetoacetate arylate or phenylazonaphthyl series. The monoazo dyes may contain further substituents which are of the kind conventionally used in azo dyes and which do not react with polycarbonate. Other dyes suitable for use in the present invention are anthraquinone dyes. Preferred dyes are selected from the group consisting of: solvent green 3, solvent green 28, solvent green 38, solvent red 52, solvent red 101, solvent red 111, solvent red 135, solvent red 169, solvent red 179, solvent red 207, disperse red 22, vat red 41, solvent orange 60, solvent orange 63, disperse orange 47, solvent violet 13, solvent violet 14, solvent violet 36, solvent violet 50, disperse violet 26/31, disperse blue 73, solvent blue 97, solvent blue 101, solvent blue 104, solvent blue 122, solvent blue 138, disperse yellow 201, solvent yellow 33, solvent yellow 114, solvent yellow 93, solvent yellow 98, solvent yellow 163, solvent yellow 160:1, solvent yellow 188, and mixtures of at least two of the foregoing colorants. These colorants are compatible with the polycarbonate-containing polymer composition and are well soluble and/or dispersible in mold release agents such as pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate, and mixtures thereof.
In a preferred embodiment, the colorant is selected from the group consisting of: solvent green 3, solvent green 28, solvent green 38, pigment green 50, pigment green 36, solvent red 52, solvent red 101, solvent red 111, solvent red 135, solvent red 169, solvent red 179, solvent red 207, pigment red 101, disperse red 22, vat red 41, solvent orange 60, solvent orange 63, disperse orange 47, solvent violet 13, solvent violet 14, solvent violet 36, solvent violet 50, disperse violet 26/31, pigment blue 29, pigment blue 60, copper phthalocyanine pigment blue 15.4, phthalocyanine blue BN, pigment blue PB 15, disperse blue 73, solvent blue 97, solvent blue 101, solvent blue 104, solvent blue 122, solvent blue 138, pigment yellow 53, pigment yellow 138, pigment yellow 139, disperse yellow 201, solvent yellow 33, solvent yellow 114, solvent yellow 93, solvent yellow 98, solvent yellow 163, solvent yellow 160:1, solvent yellow 188, pigment brown 24, aminoketone black, chromium oxide, and mixtures of at least two of the foregoing colorants. These colorants are compatible with the polycarbonate-containing polymer composition and are well soluble and/or dispersible in mold release agents such as pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate, and mixtures thereof.
The composition does not contain carbon-based pigments such as carbon black, channel black, or pigment black 6.
The colorant can be a single dye, a mixture of dyes, a single pigment, a mixture of pigments, or a mixture of one or more dyes and one or more pigments.
In the field of polymer compositions, release agents are considered to be substances which make it easier for articles prepared from polymer compositions containing said release agents to release from surfaces than from otherwise identical polymer compositions which do not contain release agents. For example, mold release agents are commonly employed in polymer compositions for making injection molded articles. The mold release agent allows the injection molded article to be removed from the mold more easily, i.e., with less force. For articles prepared by extrusion, the release agent allows for improved release from a surface, such as a surface like a calender roll or chill roll, or reduced friction with the surface.
The skilled person will appreciate that the type of release agent employed depends on the type of polymer.
In the context of the present invention, the mold release agent has a melting point sufficiently above room temperature to allow it to be used as a solid substance in a production environment. Preferably, the release agent has a melting point of at least 50 deg.C, preferably 50-100 deg.C, more preferably 50-85 deg.C. In this context, it is to be noted that the melting ranges of pentaerythritol tetrastearate, glycerol monostearate and glycerol tristearate are 60-66 ℃, 57-65 ℃ and 72-75 ℃ respectively.
The use of these mold release agents in combination with compositions comprising or consisting of polycarbonate as polymer is known, for example, from WO2014/203173 and WO 2015/132740.
According to the invention, the mould release agent is pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate or a mixture of at least two of these mould release agents. That is, in the context of the present invention, the mold release agent is selected from the group consisting of pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate and mixtures thereof. Thus, the release agent may be pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate, or a mixture of pentaerythritol tetrastearate and glycerol monostearate, a mixture of pentaerythritol tetrastearate and glycerol tristearate, or a mixture of glycerol monostearate and glycerol tristearate, or a mixture of pentaerythritol tetrastearate, glycerol monostearate and glycerol tristearate.
For the avoidance of doubt, it is noted that the substance "pentaerythritol tetrastearate" is to be understood as the substance registered under CAS number 115-83-3.
In the context of the present invention, a mold release composition is a composition in particulate form (at room temperature) and contains a colorant and at least 40 wt%, such as 40-99 wt% or 50-95 wt%, of a mold release agent, based on the weight of the mold release composition. The composition is preferably in the form of pellets, powder, beads or flakes. Such forms are known to the skilled person.
The release agent acts as a carrier material for the colorant. And the colorant is dissolved in the release agent. The mold release composition may also contain other functional additives such as UV stabilizers, antioxidants, hydrolytic stabilizers, flame retardants, catalyst quenchers, antistatic agents, and the like. The catalyst quencher is a substance that deactivates the catalyst remaining in the polymer after polymerization. In embodiments where the polymer is a polycarbonate prepared using a melt transesterification process, the preferred catalyst quencher is butyl tosylate.
Preferably, the mold release composition comprises at least 40 wt.%, more preferably at least 50 wt.%, of the mold release agent, based on the weight of the mold release composition. The amount of colorant depends on the desired hue of the final article, but can be from 0.0001 to 0.1 weight percent based on the weight of the mold release composition.
For the avoidance of doubt, the release agent composition does not comprise a carrier resin or carrier polymer.
In the process for preparing a colored polymer composition according to the present invention, the solid form of the release agent consists of one or more of pellets, powder, flakes or beads.
The mold release composition may be prepared by mixing the mold release agent, the colorant, and optionally other functional additives at a temperature above the melting temperature of the mold release agent. Mixing allows the preparation of a homogeneous mixture which is continuously cooled to a temperature below the melting temperature of the release agent and shaped into a particulate form such as pellets, powder, beads or flakes using generally known techniques. In an alternative method of preparing the mold release composition, the mold release composition is divided into droplets at a temperature above the melting temperature of the mold release agent, after which the mold release composition is cooled to a temperature below the melting temperature of the mold release agent. Depending on the droplet size, this embodiment directly produces a powder, bead or pellet. By allowing the droplets to cool on the surface, pellets or beads having one flat surface and one rounded surface can be obtained. The resulting sheet is made in a known manner, such as by cooling the molten mold release composition on a chill roll, after which the composition solidifies and is scraped to form a sheet.
In a preferred embodiment, the mold release composition comprises or consists of:
-at least 60.0% by weight of a mould release agent selected from pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate or a mixture of at least two of the aforementioned mould release agents,
-0-40% by weight of UV stabilizers,
-0.0001 to 0.1% by weight of at least one dye soluble in the mould release agent,
wherein the amounts are based on the total weight of the mold release composition and the mold release composition amounts to 100 wt.%.
The coloured polymer composition is prepared using a melt mixing device, preferably an extruder. The extruder is provided with a feed section to feed the release agent composition in solid form to the extruder. The polymer may be fed to the extruder in solid or molten form. For example, the polymer may be fed to the feed section of the extruder in the form of powder, beads or pellets. The location of the polymer feed zone may be the same as or different from the feed zone of the mold release composition. It is also possible to premix the mold release composition in solid form and the polymer in solid form and then feed the solid mixture thus obtained to the feed section of the extruder. The molten stream of polymer may be fed to the extruder via a separate feed system. The melt stream can be obtained by means of a further extruder in which the polymer is melted and extruded into a melt mixing device in which a mold release agent in solid form is added. Alternatively, the molten stream of polymer originates from a final reactor in a polymer plant, such as, for example, a melt polycarbonate plant. The colored polymeric composition formed in the extruder may be extruded through an extrusion die, cooled, and cut into pellets.
The colored polymeric compositions can be used to make semi-finished or finished articles by known conversion techniques including, but not limited to, injection molding, blow molding, sheet extrusion, profile extrusion, rotational molding, and compression molding.
In one embodiment, the extruder is connected to an injection mold and the molten pigmented polymer composition is used directly to make the final injection molded article or a semi-finished injection molded article (batch). In another embodiment, an extruder is connected to an extrusion die and the molten pigmented polymer composition is used directly to make a final extruded article or a semi-finished extruded article, such as a sheet, panel, profile, multi-wall panel, and the like.
The invention further relates to a coloured polymer composition obtained or obtainable by the process of the invention. In particular, the present invention relates to a coloured polymer composition comprising a polymer, a mould release agent and a colourant obtained or obtainable by a process comprising the steps of: feeding a mold release composition comprising the mold release agent and the colorant in solid form to a feed section of a melt mixing device; feeding the polymer to the melt mixing device; and mixing the mold release composition and the polymer in the melt mixing device at a temperature above the melting temperature of the polymer; wherein the polymer is a polycarbonate and the mold release agent is selected from the group consisting of pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate and mixtures thereof, preferably pentaerythritol tetrastearate.
The color values (dE, L, a, b) were calculated according to ASTM E308-15(Standard Practice for calculating the Colors of Objects by Using the CIE System) Using D65 illumination and spectral transmission data from a 10 ℃ observer. The transmission spectra can be collected on an X-rite i7 spectrophotometer. The color difference is calculated according to the CIE 1976 color difference equation:
Figure BDA0002816325260000101
wherein:
color difference dE ═ color difference
difference of dL-value from reference L-value
difference of da ═ a ═ from reference a ═ value
difference of db (b) value compared to reference b (b) value
Color measurements were carried out on injection-molded plates having a thickness of 4 mm.
The colored polymer composition preferably has an average dE value of at most 0.050, wherein the dE value is calculated using the above formula, and wherein said average dE value is determined for an amount of colored polymer composition between 2000 and 5000kg, and wherein the color values (L, a, b) of at least 10 and at most 20 samples are measured at regular intervals during the manufacture of said amount. The reference for determining dE for each sample consists of the average L, a and b calculated on the basis of all measurements within the amount of coloured polymer composition.
Examples
The invention will now be further described in detail based on the following non-limiting examples.
The following mold release compositions, designated a and B, were prepared by: the ingredients are mixed at a temperature of about 70 ℃ followed by forming nearly round shaped pellets from the molten release agent composition by cooling the droplets of the molten composition on a flat surface. The pellets have a diameter of about 3mm and a maximum thickness of between about 1 and 2 mm.
The amount is in parts by weight. Compositions a and B do not contain any other substances. For each of compositions A and B, the sum of the weights of the components in Table 1 totals 100 parts by weight.
TABLE 1
Figure BDA0002816325260000111
Based on the starting materials and the mold release compositions a and B, the following colored polymer compositions were prepared. All example polymer compositions were prepared using a co-rotating twin screw extruder with the same settings. The extruder length was 2880mm (8 barrels) and the screw diameter was 92mm, operating at a screw speed of 600rpm, yielding an output of about 2500 kg/hr. The barrel temperature over the wetted length and the temperature of the die were set to 300 ℃. The extruder was equipped with a bulk feeder for feeding the polymer in powder form, a blend feeder for feeding the blend of the individual components of comparative examples 1 and 2, and a pellet feeder for feeding the pellets of compositions a and B. The bulk feeder, blend feeder, and pellet feeder all feed each to the same feed section in the extruder at the first barrel. The colored polymer composition is extruded into strands, which are cooled and cut into pellets.
Samples of the resulting pellets were withdrawn at regular intervals during the preparation of the composition. These samples were dried and injection molded into sets of 5 plates of approximately 6cm by 6cm and 4mm thickness.
The color of the plates was measured using a color spectrophotometer using the CieLAB system to generate values for L, a, b for each plate. For purposes of the examples in this application, the values of L, a, and b for each sample are the average of 5 plates per sample.
For the calculation of dE, the reference consists of the average of L, a and b, all based on all plates measured within the example composition.
The average dE reported in table 3 below is the average of all individual dE measurements within the example compositions.
The maximum dE reported represents the dE value of the sample with the highest measured color difference.
Thus, in comparative example 1(CE1), 16 samples were taken at regular intervals during the preparation of the colored polymer composition. Five plates of 4mm thickness were prepared from each of these 16 samples via injection molding. Using the CIElab system, each panel was subjected to color measurements, resulting in a data set of 16 by 5 individual color measurements. The average color values of L, a and b form the reference values for calculating dE according to the above formula.
TABLE 2
Figure BDA0002816325260000131
The polycarbonates fed via the bulk feeder and via the blend feeder were identical and consisted of polycarbonate having an Mw of about 30500 g/mol (PC standard) and about 6.0 cm3A melt volume flow rate of 10min (ISO 1133, 300 ℃, 1.2 kg). The polycarbonate was prepared using an interfacial process in which bisphenol a was reacted with phosgene, and the resulting polymer powder was fed to the bulk and blend feeders of the extruder.
Table 3 shows the color change as a result of measurement on the board prepared by example.
TABLE 3
CE1 CE2 E1 E2
Number of samples in batch 16 24 25 19
Average dE- 0.088 0.072 0.032 0.047
Maximum dE 0.2 0.166 0.076 0.122
The results in table 3 show that the color change of the molded plate, i.e., the article, can be significantly reduced after using the mold release composition containing the colorant. The inventors believe that this observed improved color consistency means that the concentration of colorant in articles made from the polymer composition shows less variation.

Claims (14)

1. A process for preparing a colored polymer composition comprising a polymer, a mold release agent, and a colorant, the process comprising the steps of: feeding a mold release composition comprising the mold release agent and the colorant in solid form to a feed section of a melt mixing device; feeding the polymer to the melt mixing device; and mixing the mold release composition and the polymer in the melt mixing device at a temperature above the melting temperature of the polymer, wherein:
-the colorant is a pigment or dye soluble in the release agent,
-the polymer composition comprises or consists of polycarbonate,
-said mould release agent is selected from the group consisting of pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate and mixtures thereof.
2. The method of claim 1, wherein the colorant is a dye.
3. The method of claim 1 or 2, wherein the solid form of the release agent consists of one or more of pellets, powder, flakes, or beads.
4. The method of any one or more of claims 1-3, wherein the mold release composition further comprises one or more functional additives selected from the group consisting of antioxidants, UV stabilizers, hydrolysis stabilizers, flame retardants, catalyst quenchers, antistatic agents.
5. The method of any one or more of claims 1-4, wherein the mold release composition comprises at least 40.00 wt% of a mold release agent, based on the weight of the mold release composition.
6. The method of any one or more of claims 1-5, wherein the polymer comprises at least 60 wt.%, preferably at least 80 wt.%, more preferably at least 90 wt.%, of polycarbonate, based on the weight of the polymer.
7. The method of any one or more of claims 1-6, wherein the polymer consists of an aromatic polycarbonate or a mixture of at least two aromatic polycarbonates.
8. The method of any one or more of claims 1-7, wherein the melt mixing device is an extruder.
9. The method of any one or more of claims 1-8, further comprising the step of preparing the mold release composition by mixing the mold release agent and the colorant, and optionally one or more functional additives selected from the group consisting of antioxidants, UV stabilizers, hydrolytic stabilizers, flame retardants, catalyst quenchers, and antistatic agents, at a temperature above the melting temperature of the mold release agent.
10. A process for manufacturing a semi-finished article or a batch of final articles, said process comprising converting a coloured polymer composition obtained or obtainable by a process according to any one or more of claims 1 to 9 into said article by means of injection moulding, blow moulding, rotational moulding, compression moulding, sheet extrusion or profile extrusion.
11. Use of a mold release composition comprising a mold release agent and a colorant in particulate form for preparing a colored polymer composition by melt mixing a polymer and the mold release composition at a temperature above the melting temperature of the polymer, wherein:
-the colorant is a pigment or dye soluble in the release agent,
-the polymer comprises or consists of polycarbonate,
-said mould release agent is selected from the group consisting of pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate and mixtures thereof.
12. The use according to claim 11 for improving the color consistency of articles prepared from the pigmented polymer composition.
13. A mold release composition comprising at least 40% by weight of a mold release agent and at least 0.0001% by weight of a colorant, wherein the mold release agent is in particulate form, preferably in the form of pellets, powder, beads or flakes, wherein the colorant is a pigment or dye soluble in the mold release agent, and the mold release agent is selected from the group consisting of pentaerythritol tetrastearate, glycerol monostearate, glycerol tristearate and mixtures thereof.
14. The method of any one or more of claims 1-10, the use of claim 11 or 12, or the mold release composition of claim 13, wherein the colorant is selected from the group consisting of: solvent green 3, solvent green 28, solvent green 38, pigment green 50, pigment green 36, solvent red 52, solvent red 101, solvent red 111, solvent red 135, solvent red 169, solvent red 179, solvent red 207, pigment red 101, disperse red 22, vat red 41, solvent orange 60, solvent orange 63, disperse orange 47, solvent violet 13, solvent violet 14, solvent violet 36, solvent violet 50, disperse violet 26/31, pigment blue 29, pigment blue 60, copper phthalocyanine pigment blue 15.4, phthalocyanine blue BN, pigment blue PB 15, disperse blue 73, solvent blue 97, solvent blue 101, solvent blue 104, solvent blue 122, solvent blue 138, pigment yellow 53, pigment yellow 138, pigment yellow 139, disperse yellow 201, solvent yellow 33, solvent yellow 114, solvent yellow 93, solvent yellow 98, solvent yellow 163, solvent yellow 160:1, solvent yellow 188, pigment brown 24, aminoketone black, chromium oxide, and mixtures of at least two of the foregoing colorants.
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